#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/37/2013791.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2013791 loop_ _publ_author_name 'Bruce, Michael I' 'Head, Nicholas J.' 'Skelton, Brian W.' 'White, Allan H. ' _publ_section_title ; 1,4-Diethynyl-2,5-dimethoxybenzene at ca 150 K ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first o60 _journal_page_last o61 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C12 H10 O2' _chemical_formula_moiety 'C12 H10 O2' _chemical_formula_sum 'C12 H10 O2' _chemical_formula_weight 186.21 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00000 _cell_angle_beta 106.710(2) _cell_angle_gamma 90.00000 _cell_formula_units_Z 2 _cell_length_a 9.1110(10) _cell_length_b 5.9921(7) _cell_length_c 9.4080(10) _cell_measurement_reflns_used 3004 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 34.6 _cell_measurement_theta_min 2.8 _cell_volume 491.93(9) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'Xtal3.5 (Hall et al., 1995)' _computing_molecular_graphics Xtal3.5 _computing_publication_material 'BONDLA and CIFIO in Xtal3.5' _computing_structure_refinement 'CRYLSQ in Xtal3.5' _computing_structure_solution Xtal3.5 _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 1.0 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measurement_device_type 'Bruker SMART CCD' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'sealed tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .025 _diffrn_reflns_av_sigmaI/netI .06 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10271 _diffrn_reflns_theta_full 37.4 _diffrn_reflns_theta_max 37.4 _diffrn_reflns_theta_min 2.33 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .085 _exptl_absorpt_correction_T_max .93 _exptl_absorpt_correction_T_min .77 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 196 _exptl_crystal_size_max .35 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .08 _refine_diff_density_max .527 _refine_diff_density_min -.206 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_constraints 0 _refine_ls_number_parameters 84 _refine_ls_number_reflns 1957 _refine_ls_number_restraints 0 _refine_ls_R_factor_all .062 _refine_ls_R_factor_gt .044 _refine_ls_shift/su_max .005 _refine_ls_shift/su_mean .001 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.0003F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .054 _refine_ls_wR_factor_ref .05 _reflns_number_gt 1957 _reflns_number_total 2574 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gd1290.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_cif_authors_sg_Hall '-p 2ybc' _cod_database_code 2013791 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z -x,1/2+y,1/2-z -x,-y,-z +x,1/2-y,1/2+z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 .12902(9) .11388(15) .08619(9) .0184(3) Uani ? ? 1.00000 ? ? C11 .26167(10) .22987(15) .17564(10) .0206(3) Uani ? ? 1.00000 ? ? C12 .37230(11) .32442(18) .25064(11) .0253(4) Uani ? ? 1.00000 ? ? C2 .14706(9) -.07129(15) .00091(9) .0185(3) Uani ? ? 1.00000 ? ? O2 .29445(7) -.12925(12) .01094(7) .0232(3) Uani ? ? 1.00000 ? ? C21 .31587(11) -.30991(18) -.08093(11) .0251(4) Uani ? ? 1.00000 ? ? C3 .01834(9) -.18351(15) -.08506(9) .0199(3) Uani ? ? 1.00000 ? ? H12 .4603(18) .398(3) .3090(17) .043(4) Uiso ? ? 1.00000 ? ? H21a .4284(16) -.323(2) -.0608(15) .032(3) Uiso ? ? 1.00000 ? ? H21b .2691(16) -.275(2) -.1866(15) .030(3) Uiso ? ? 1.00000 ? ? H21c .2737(14) -.450(2) -.0564(14) .028(3) Uiso ? ? 1.00000 ? ? H3 .0288(14) -.312(2) -.1451(14) .025(3) Uiso ? ? 1.00000 ? ? loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 C1 .0136(3) .0204(4) .0185(3) .0000(3) .0003(2) -.0007(3) C11 .0168(3) .0220(4) .0214(4) .0011(3) .0028(3) -.0002(3) C12 .0189(4) .0276(4) .0266(4) -.0024(3) .0020(3) -.0029(3) C2 .0125(3) .0219(4) .0190(3) .0020(3) .0011(2) .0000(3) O2 .0132(2) .0290(3) .0250(3) .0036(2) .0019(2) -.0053(3) C21 .0214(4) .0273(4) .0264(4) .0056(3) .0068(3) -.0025(3) C3 .0151(3) .0217(4) .0205(3) .0011(3) .0012(2) -.0034(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 C11 . . 1.4377(11) ? C1 C2 . . 1.4063(13) ? C1 C3 . 3 1.4031(12) ? C11 C12 . . 1.1941(12) ? C12 H12 . . .940(14) ? C2 O2 . . 1.3638(11) ? C2 C3 . . 1.3914(11) ? O2 C21 . . 1.4331(13) ? C21 H21a . . .991(15) ? C21 H21b . . .985(13) ? C21 H21c . . .979(14) ? C3 H3 . . .974(14) ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1' H 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1' O .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle C11 C1 C2 . 119.93(8) C11 C1 C3 3 120.15(8) C2 C1 C3 3 119.92(7) C1 C11 C12 . 179.39(11) C11 C12 H12 . 179.1(11) C1 C2 O2 . 115.83(7) C1 C2 C3 . 119.71(8) O2 C2 C3 . 124.45(8) C2 O2 C21 . 116.92(7) O2 C21 H21a . 104.9(8) O2 C21 H21b . 110.7(8) O2 C21 H21c . 112.1(9) H21a C21 H21b . 109.4(12) H21a C21 H21c . 110.0(11) H21b C21 H21c . 109.6(11) C2 C3 H3 . 120.8(7) C2 C3 C1 3 120.36(8) H3 C3 C1 3 118.9(7) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag C12 H12 O2 2_655 0.940(10) 2.390(10) 3.2270(10) 148.0(10) yes _cod_database_fobs_code 2013791 _journal_paper_doi 10.1107/S0108270103027124